Lab Report 1: Steam Distillation Introduction: The purpose of this experiment was to isolate eugenol or clove oil from cloves using steam distillation and determine whether it is an efficient way to carry out this experiment. Also, TLC and 1H NMR were preformed to analyze the purity of the isolated eugenol. Theory: Steam distillation uses boiling point to separate organic liquid and water. The organic compound must be immiscible with water, have a high vapor pressure at 100˚C, and may decompose before boiling point is reached. Steam distillation increases the vapor pressure of water more than the vapor pressure of the organic compound as temperature rises to reach the boiling point of the mixture which is a little less than 100 ˚C (boiling point of water) but a lot less than 254 ˚C (boiling point of eugenol). Since the liquids are immiscible, the total vapor pressure only depends on the vapor pressure of each component added together and not the mole fraction leading to a higher vapor pressure which corresponds to the lower boiling point. Extraction separates compounds based on their solubility. A separatory funnel allows two distinct layers (aqueous and organic) to form when two immiscible liquids are separated with the more dense liquid on bottom. In this lab, dichloromethane (organic) has a density of 1.33g/mL while water (aqueous) has the density of 1.00g/mL, so dichloromethane will be on the bottom and since “like dissolves like” and eugenol does not dissolve in water but dissolves in dichloromethane, eugenol will be found in the dichloromethane layer. TLC allows identification of compounds based on polarity. Nonpolar compounds move higher up on the TLC plate than polar compounds because polar compounds are more attracted t... ... middle of paper ... ..., and is immiscible with water. Since there was not clear distinct two layers after steam distillation, extraction was used to separate the eugenol from water thus, steam distillation is not an effective way to isolate eugenol by itself. In order to determine how pure the isolated eugenol was, TLC was performed and compared to the standard and 1H NMR of the isolated eugenol and standard were compared to conclude that the extracted compound was eugenol with some impurities. Appendix: Mass of Eugenol: Mass of Vial + Eugenol- Mass of Vial= 16.498g-16.429g=0.069g Theoretical Mass of Eugenol: Mass of Eugenol/ Total Mass of Cloves x 100= Mass % x/4.976 x 100=17% x/4.976=0.17 x=4.976x0.17=0.85g Percent Recovery: Actual Mass/Theoretical Mass X100= 0.069g/0.85g x100= 8.12% Rf Value Rf= Origin to Center of Spot/ Origin to Solvent Front Line= 1.5cm/5.3cm=0.28 3.4 cm/5.3cm=0.64
Esters are defined as molecules consisting of a carbonyl group which is adjacent to an ether linkage. They are polar molecules which are less polar than alcohols but more so than ethers, due to their degree of hydrogen bonding ability. Most often derived from reacting an alcohol with a carboxylic acid, esters are a unique, ubiquitous class of compounds with many useful applications in both natural and industrial processes 1. For example, within mammals, esters are used in triglycerides and other lipids as they are the main functional group attacking fatty acids to the glycerol chain 2. A unique property of esters is their tendency to give off distinct aromas such as the scent of apples (Ethyl caprylate) and bananas (Isoamyl acetate). This is of a unique importance especially in industries that utilize flavors and aromas such as the tobacco, candy and alcohol industry. Consistent research is conducted in order to enhance and increase the effectiveness of esters in these products 3.
The objective of this experiment was to perform extraction. This is a separation and purification technique, based on different solubility of compounds in immiscible solvent mixtures. Extraction is conducted by shaking the solution with the solvent, until two layers are formed. One layer can then be separated from the other. If the separation does not happen in one try, multiple attempts may be needed.
Distillation uses the characteristic boiling points of pure liquids to separate these substances from a mixture. Once a pure liquid reaches its boiling point, it maintains this temperature as
This report will outline the steps taken to design a packed distillation column. The column needs to separate a 50:50 mixture of ethanol and isopropanol into a distillate stream containing no more than 3 wt% isopropanol and a bottoms stream containing no more than 3 wt% ethanol. The design of the full-scale column was based on a laboratory simulation column. This column allowed the team to determine vapor velocities and HETP values for the 0.24 inch Pro-Pakq packing.
Because of the limited amount of time the student is provided during this lab experiment, the complete amount of distillate was not collected fully due to the procedure being very slow and time consuming. The final eugenol that was isolated was not completely pure, and this is proven by the percent recovery being 110%, which is clearly higher than a 100%. This means that other substances were isolated along with the eugenol oil, such as leftover dichloromethane, which was used in the first place because the water and eugenol did not successfully separate into two layers, thus dichloromethane was added to help separate them. This is was caused percent recovery to be higher than what it should be. Heating and boiling the final solution for a longer time until all the dichloromethane is evaporated completely can easily avoid the presence of
This difference is that eugenol has a alcohol group (OH) coming off its benzene ring while acetyleugenol has an ester group coming off its ring instead. This important stuctural difference is what allowed the separation between eugenol and acetyleugenol. This can be seen during extraction when the sodium hydroxide was added to the methylene chloride layer containg the eugenol and acetyleugenol. The OH group on the eugenol is able to react with the sodium hydroxide as seen in the mechanism diagram above. This reaction leads to eugenol going into the sodium hydroxide layer while the acetyleugenol is left in the methylene chloride layer. The eugenol’s OH group reacts with the negativle charged OH from the NaOH. The reaction leads to the eugenol’s OH group becoming a negativly charged oxygen. This negativley charged oxygen then reacts with the positivly charged Na from the NaOH and forms an eugenol salt. Eugenol salts dissolve in water, thus allowing the eugenol to be take from the sodium hydroxide layer to the water. The acetyleugenol has an ester group instead of an OH group, so it cannot under go this same extraction
Title: Sterilization by Saturated Steam Introduction: The sterilization process is done to completely eliminate all microorganisms that could potentially be a contaminant and lead to occurrences of hazards (Chi, 1993). Sterilization is a process defined by killing all living microorganisms, including bacteria and spores. This process can be done chemically, physically, and by means of physiochemical methods (Soper & Davies, 1990). Chemicals used in these processes to ensure all microorganisms no longer exist are known as sterilizing agents and are called chemisterilants.
A mixture of solvent is used when the solvent does not have the wanted properties of rendering the soluble when how and insoluble when cold. Suction filteration causes crystals to clog the funnel, which is why gravity filtration is prefered. Fluted filter paper is used becuae it has a larger surface area making it easier for solvent to flow. Stemless funnels are used because the long-stem funnels will cool which will cause clogging of thr steam due to the crystals. Vacuum filtration is more effective for removing solvsent from the crystals than the gravity filtration.
Packed distillation column is where miscible liquids are separate accordicaly to physical, specifically or volatilities of the compounds. Liquids can categories as volatile when it vaporized in low temperature. The more boiling of volatile compounds of mixture through the distillation process if the vapor is cooler the volatile material condenses in a proper proportion than less volatile compounds. Packed distillation column gives a situation where the gas and liquid phases of each material can approach the equilibrium level. A column can have packing or trays, in this columns increase in surface areas can
Once the mixture had been completely dissolved, the solution was transferred to a separatory funnel. The solution was then extracted twice using 5.0 mL of 1 M
Fractional distillation is the separation of a liquid mixture into its different fractions; fractions are the different parts of a mixture. In this case we went through and boiled our mixture to find the plateau of the substances in the mixture. A plateau is a state of little to no change after a time of progress. We also used filtration by evaporation which is used to separate a soluble solid from a liquid. Throughout this investigation we watched for the characteristic properties and to check the solubility we used solute and solvent.
After performing the first Gas Chromatography, we took the organic layer, and mixed it with saturated Sodium Hydroxide. We performed this step to remove the (-OH) group from the Eugenol. The purpose was to make the water as a product, which can also be used as a solvent for the Eugenol that was ionized, for the two substances Acetyl Eugenol and Beta Caryophyllene. Again, we see the density differences in the solvents; we were able to take the organic layer. Finally, we transferred the layer into the beaker and dried, to perform the Gas Chromatography
Eugenol was extracted from cloves through the process called steam distillation. A total of 50ml of distillate were collected with temperature monitoring for every 5.0ml of collected liquid. The distillation curve showed that the temperature of volatilization of eugenol is from 98°C to 99°C which is way below its boiling point at 2540C. Chemically active extraction was conducted in order to remove impurities particularly eugenol acetate and caryophyllene. This involves the addition of several solvents particularly hexane, NaOH, HCl, then hexane again in succession.
the separation of large solids and fluids, by means of a filter (Lenntech, n.d.). The
First of all, the purpose of this lab was to determine the water’s vapor pressure at different temperatures as well as to measure the molar heat of vaporization of water using the Clausias Clapeyron equation. The first concept out of many represented in this lab is the ideal gas law. The ideal gas law is used to get the number of moles of air trapped in the 10 mL graduated cylinder. Once we cooled the system so that water vapor is extremely minute, and then we determined the number of moles of air using the ideal gas law. The number of moles of air equals to the pressure (in atm) times volume divided by constant times temperature. One would assume that when the water is heated to 80 degrees, the number of air molecules in the air bubble would decrease, but it actually stays constant. This is due to the fact that there is no air coming in or out of the cylinder. As the temperature gets closer to 80 degrees, the number of air molecules stays the same but the water vapor increases. And the bubble expands to keep the pressure at the same level. The ideal gas law was also used when the partial pressure of air in the gas mixture is calculated. This is gotten from number of moles multiplied by the constant and the constant and the whole thing divided by the volume.